WO2017217804A1 - Appareil et procédé de mesure de contaminants ioniques sur la surface d'une tranche - Google Patents

Appareil et procédé de mesure de contaminants ioniques sur la surface d'une tranche Download PDF

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Publication number
WO2017217804A1
WO2017217804A1 PCT/KR2017/006313 KR2017006313W WO2017217804A1 WO 2017217804 A1 WO2017217804 A1 WO 2017217804A1 KR 2017006313 W KR2017006313 W KR 2017006313W WO 2017217804 A1 WO2017217804 A1 WO 2017217804A1
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sample
wafer
scanning
measuring
ionic
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PCT/KR2017/006313
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English (en)
Korean (ko)
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이응선
유승교
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주식회사 위드텍
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Publication of WO2017217804A1 publication Critical patent/WO2017217804A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/10—Measuring as part of the manufacturing process
    • H01L22/12—Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/8851—Scan or image signal processing specially adapted therefor, e.g. for scan signal adjustment, for detecting different kinds of defects, for compensating for structures, markings, edges
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/94—Investigating contamination, e.g. dust
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
    • H01L22/24—Optical enhancement of defects or not directly visible states, e.g. selective electrolytic deposition, bubbles in liquids, light emission, colour change
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/30—Structural arrangements specially adapted for testing or measuring during manufacture or treatment, or specially adapted for reliability measurements

Definitions

  • the present invention relates to an apparatus and method for measuring ionic contaminants on a wafer surface, and more particularly, to collect contaminants that are present on a wafer surface during a semiconductor process through a wafer surface scan, and in the collected solution, such as NH 4 + and Cl ⁇ .
  • An apparatus and method for measuring ionic contaminants on a wafer surface capable of measuring and analyzing ionic components.
  • ionic components such as NH 4 + and Cl ⁇ may not only remain on the surface of the wafer from chemicals used in the process, but may also be contaminated in air and remain on the surface. Since these ionic contaminants are conductive, they have a more serious effect when present above the control level, so very low concentration control is required.
  • VPD a method of measuring pollutants after removing an oxide film from a wafer surface using VPD, such as VPD-ICP-MS, VPD-TXRF, and VPD-AAS, is used as a measurement technique or measuring equipment on a wafer surface.
  • these methods remove the oxide film from the wafer surface by using HF, H2O2, HCl, H2SO4 as liquid droplets and decomposition by HF, so it is possible to analyze metal components on the wafer. Due to the very large dilution, it is impossible to measure the trace concentration, the system for analysis becomes complicated, and parts damage and aging due to a large amount of chemical are rapidly progressed.
  • the oxide film is removed using a droplet solution of HF
  • a large amount of HF is present in the sample extracted from the wafer, and it is almost impossible to measure impurities for F- ions on the wafer.
  • impurities such as Cl-
  • the system becomes complicated and difficult to measure precise concentrations, because a large amount of dilution has to be measured in advance due to the interference of a large amount of F- and damage to the measuring device. In case of a small amount, the detection is not easy.
  • the present invention has been made to solve the above problems, an object of the present invention is to automatically scan the surface of the wafer to be analyzed to collect ionic contaminants, and to automatically measure and analyze the ionic components of the collected material It is to provide a new device and method.
  • the present invention collects contaminants present on the wafer surface during the semiconductor process to measure ionic contaminants on the wafer surface by scanning the wafer surface, and by measuring and analyzing ionic components such as NH 4 + and Cl ⁇ in the collected solution.
  • ionic components such as NH 4 + and Cl ⁇
  • ionic contaminants such as NH 4 + and Cl ⁇ remain on the wafer surface from the chemicals used in the process or from the air.
  • the contamination measurement device of the conventional wafer surface removes the oxide film on the wafer surface by using HF, H 2 O 2, HCl, H 2 SO 4 as a liquid droplet and decomposition by HF, it is possible to analyze metal ions on the wafer.
  • a great deal of dilution is required due to matrics effects. As a result, the system becomes complicated, it is difficult to measure precise concentrations, and in the case of a trace amount, it is difficult to detect it.
  • the present invention is a measuring device and measuring method for the purpose of measuring and analyzing the ionic contaminants present on the wafer surface, there is an advantage that can effectively analyze the ionic components compared to the conventional device.
  • contaminant monitoring can be performed in near real time, greatly reducing production defects in semiconductor devices.
  • the present invention has an effect that can prevent data loss by automatically storing the sample when the analysis is impossible or when the analysis conditions are incorrect and difficult to accurately analyze.
  • FIG. 1 is a schematic configuration diagram of an ionic contaminant measuring device according to an embodiment of the present invention
  • Figure 2 is a block diagram showing a method for measuring ionic contaminants in accordance with an embodiment of the present invention
  • FIG. 3 is a cross-sectional view briefly showing the operation of the wafer scanning unit according to an embodiment of the present invention.
  • FIG. 4 is a cross-sectional view schematically showing still another operation of the wafer scanning unit according to an embodiment of the present invention.
  • FIG. 5 illustrates various embodiments of a scan nozzle cleaning method of the present invention.
  • 6 to 12 are several embodiments of the ion component measurement process of the present invention.
  • 13 and 14 are flowcharts illustrating a parameter monitoring process of the present invention.
  • 15 is a conceptual diagram schematically illustrating an operation according to another embodiment of the present invention.
  • An apparatus for measuring ionic contaminants adsorbed or remaining on a surface of a wafer during a semiconductor process includes a scan stage in which the wafer is loaded without vapor decomposition, the wafer A scanning unit for scanning and collecting ionic contaminants on the surface of the wafer using a scan nozzle when the loading unit is loaded; And an analyzing unit analyzing the ionic contaminants included in the sample solution collected by the wafer scanning unit.
  • the analysis unit may include a sample injection valve including an inflow passage into which a standard solution or a sample solution for calibration is introduced, an eluent, and a sample loop into which a sample of the standard solution or the sample solution is injected, and the sample Or a sample injection pump for transferring a standard solution or injecting the sample loop, a column into which a sample is injected from the sample injection valve to separate components in the sample, and a suppressor for lowering the conductivity of the background value of the sample; And a detector for detecting an ionic component included in a sample that has passed through the suppressor.
  • a sample injection valve including an inflow passage into which a standard solution or a sample solution for calibration is introduced, an eluent, and a sample loop into which a sample of the standard solution or the sample solution is injected, and the sample
  • a sample injection pump for transferring a standard solution or injecting the sample loop, a column into which a sample is injected from the sample injection valve to separate components in the sample,
  • the wafer scanning unit transfers or rotates the scan nozzle for scanning the wafer surface in a state in which the scan solution formed in the nozzle is in contact with the surface of the wafer, and the scan nozzle in any one or more of X, Y, and Z axis directions. It can be made including a scanning arm.
  • the wafer scanning unit may further include an aligner for aligning the positions of the wafers, and load the aligned wafers in the scan stage.
  • the wafer scanning unit may change the direction of the wafer or the scan nozzle such that the nozzle axis and the wafer plane are horizontal or vertical when scanning and collecting ionic contaminants present on the side of the wafer.
  • the analysis unit may further include a sample reservoir in which a predetermined amount of the sample solution introduced from the inflow oil is filled by the loading operation of the sample injection pump, and the sample solution stored by the drain operation of the sample injection pump is introduced and stored. It can be done by.
  • the analyzer may further include a nozzle cleaner configured to clean the scan nozzle when the sample solution collected in the scan nozzle is transferred to the analyzer.
  • the analysis unit may further comprise a two-way valve or more to clean the syringe pump and the flow path.
  • the analyzer may inject a sample into the injector after loading the sample solution introduced from the inflow oil by the loading operation of the sample injection pump.
  • the analyzer may include at least one or more flow paths between the sample injection valve and the sample injection pump, and further include a flow control valve for controlling fluid flow in two or more directions.
  • the analysis unit is provided with a plurality of standard solution injector for injecting the standard solution of different concentrations, or a plurality of sample reservoirs for storing different sample solutions, respectively, the measuring device is the stop of the inflow And a selection valve for selectively communicating any one of the standard solution injector or the sample reservoir.
  • the apparatus for measuring ionic contaminants on the wafer surface of the present invention monitors various parameters based on the measured values of the sensors provided for each predetermined position of the analysis unit and the previous measurement result of the detector, and at least one of the parameters is a reference value
  • the control unit may further include a control unit for controlling each device to return to the load port without scanning the wafer or to automatically store the sample solution collected by scanning the wafer without analyzing the sample solution.
  • the sample solution is diluted with ultrapure water at a predetermined ratio and diluted, and then transferred to the column, or the sample solution is injected into a concentrated column and concentrated to transfer to the column,
  • the detector may be configured to correct the detection result by reflecting the dilution or concentration ratio in the detection result.
  • a contaminant measuring system that automatically loads the wafer in the FOUP using a robot and scans and analyzes the ionic contaminants on the wafer surface using the ionic contaminant measuring apparatus on the wafer surface of the present invention.
  • the wafer loading step is loaded on the scan stage without the gas phase decomposition;
  • the scan nozzle is moved to the nozzle cleaner to be cleaned periodically or continuously and then waiting.
  • the sample storage step of storing the sample filled in the delay coil of the analysis unit in the selected sample storage may further include a.
  • the ionic component measuring step step 2-1 in which the sample solution introduced from the inlet flow path by the sample injection pump is loaded into the delay coil; Step 2-2 in which the sample solution filled in the delay coil is introduced into the sample reservoir by the drain operation of the sample injection pump; And 2-3 steps in which the sample solution stored in the sample reservoir is measured and analyzed after a predetermined time by the analyzer, or recovered and measured and analyzed by a separate analysis device. It may be made, including.
  • step 3-1 is the ultra-pure water is loaded by the sample injection pump to the delay coil provided in the front end of the sample injection pump;
  • Step 3-2 of loading the sample solution from the wafer scanning unit when the amount of ultrapure water is loaded into the delay coil;
  • Step 3-3 of discharging the partial flow of the delay coil to the discharge passage by the drain operation of the sample injection pump and closing the discharge passage;
  • 3-7 steps of detecting the ionic component contained in the sample passing through the suppressor;
  • 3-8 in which the dilution ratio in 3-4 is reflected in the result detected in steps 3-7, thereby correcting the detection result.
  • the first monitoring step of monitoring the various parameters based on the measurement values of the sensors provided by the control unit for each predetermined position of the analysis unit and the analysis unit; In the step of monitoring, if at least one of the parameters deviates from the set reference value, the wafer is not scanned or the collected and sampled solution is analyzed without analyzing the collected sample solution by performing the scanning and collecting step, and the sample is automatically stored and stored in the sample storage. If it does not depart from the step may be performed.
  • the syringe injecting pump refers to being capable of inhaling and discharging a sample by driving the syringe, and collectively refers to whether the directional valve is attached or not.
  • FIG. 1 is a schematic configuration diagram of an ionic contaminant measuring apparatus according to an embodiment of the present invention
  • Figure 2 is a block diagram showing a ionic contaminant measuring method according to an embodiment of the present invention.
  • the present invention relates to an apparatus for measuring ionic contaminants adsorbed or remaining on a surface of a wafer during a semiconductor process.
  • the apparatus 100 includes a chamber 100, a wafer scanning unit 200, and an analysis unit. 300 and a control unit (not shown).
  • control unit is connected to each component of the ionic contaminant measuring apparatus of the present invention, and controls the respective components according to the programmed logic or the user's manual operation command.
  • the chamber 100 is provided with a door (not shown) for carrying in the wafer w to be measured, and a predetermined space is formed therein to accommodate the wafer scanning unit.
  • the load port is connected to one side of the chamber 100 to automatically transfer the FOUP in the line, and automatically take out the wafer in the FOUP and load it in the load port.
  • the contaminant is controlled in the chamber 100. That is, when the wafer w is introduced into the chamber 100, an inert gas or a high purity gas (N2, He, Clean air, etc.) without inert gas or contamination is introduced into the chamber 100 to form a gas atmosphere, and the chamber 100 The internal pressure is maintained at atmospheric or positive pressure to prevent contaminants from entering the environment.
  • a chemical filter may be installed on one surface of the chamber 100 to control the pollutants. Such contamination protection can be achieved through automatic control or manual valves.
  • the chamber 100 may be provided with a transfer robot (not shown) for the transfer of the wafer (w), the transfer robot transfers the wafer (w) when the wafer (w) is brought in from the outside through the door To be loaded onto the scan stage 210.
  • a transfer robot (not shown) for the transfer of the wafer (w)
  • the transfer robot transfers the wafer (w) when the wafer (w) is brought in from the outside through the door To be loaded onto the scan stage 210.
  • an operator may directly load a wafer onto the scan stage 210.
  • the wafer scanning unit 200 includes a scan stage 210 on which a wafer w is loaded, and scans and collects ionic contaminants on the wafer surface by using a scan nozzle when the wafer is loaded. In this case, it is preferable that the wafer loaded on the scan stage 210 is loaded without vapor phase decomposition.
  • the final analyzer 300 is a component that analyzes the ionic contaminants included in the sample solution collected by the wafer scanning unit 200.
  • Conventional pollutant analyzers vapor-decompose wafer surfaces using etching gases prior to wafer scanning. This is a process for removing the oxide film on the wafer surface to trap metal contaminants on the wafer surface.
  • the etching gas fluoric acid
  • the etching gas is used to reverse contamination with a large amount of hydrofluoric acid on the wafer, and thus accurate measurement of the ionic contaminants due to the component change of ionic components including F- ions on the wafer. This is difficult. Therefore, there is a problem that the conventional pollutant analysis device can not analyze the ionic pollutants.
  • the present invention is to measure the ionic contaminants adsorbed or remaining on the surface of the wafer during the semiconductor process, as the wafer is loaded on the scanning stage without the gas phase decomposition to perform a wafer surface scan
  • the advantage is that accurate analysis of the collected ionic contaminants is possible.
  • the measuring method according to an embodiment of the present invention is largely the wafer loading step (S100), scanning and collecting step (S200) ) And the ion component measuring step (S300).
  • the wafer loading step S100 is a step in which the wafer w brought into the chamber is loaded on the scan stage 210 without being gas-decomposed.
  • the scanning and collecting step S200 is a step in which ionic contaminants on the wafer are scanned and collected by the wafer scanning unit 200 having the scan nozzle 220, and the last ionic component measuring step S300 is analyzed.
  • step 300 the ionic components included in the sample solution are measured.
  • the wafer scanning unit 200 may include an aligner (not shown), a scan stage 210, a scan nozzle 220, and a scanning arm 230, as shown in FIG. 3A. have.
  • the aligner is configured to align the position where the wafer is loaded before the wafer is loaded on the scan stage 210, and may be selectively applied as necessary.
  • the scan stage 210 is formed so that the upper surface is flat so that the wafer (w) aligned in position can be loaded, it is configured to be rotatable about the central axis. That is, since the position of the wafer w is aligned by the aligner in the wafer loading step S100, the wafer w is placed on the scan stage 210, and then scanning may be performed on the same position. .
  • the scan nozzle 220 is configured to scan the wafer w while a scan solution formed in the form of droplets on the nozzle tip 222 is in contact with the surface of the wafer w.
  • a flow path 221 is formed to discharge the completed solution to the outside.
  • a suction pump or the like may be used to ensure that the scanning solution is bound to the nozzle tip 222.
  • by spraying a non-contaminating gas from the circumference of the nozzle tip 222 to the surface of the wafer (w) it is preferable to prevent the droplets burst or change shape due to friction with the surface during scanning to maintain the droplets continuously .
  • the shape of the nozzle tip may be variously formed, and may be diversified in a structure such that the water droplets do not burst when the wafer is scanned.
  • the flow path can also be different when injecting the solution for scanning and when transferring the scanned solution to the analyzer.
  • the scanning solution can be shaped by the shape of the droplet or the tip of the nozzle and can be used from several microliters ( ⁇ L) to several tens of milliliters (mL).
  • the scanning arm 230 may be configured to transfer or rotate the scan nozzle 220 in any one or more directions of the X, Y, and Z axes, and may be rotatable based on the column axis 231. That is, as shown, the scanning arm 230 includes a column shaft 231 formed to be rotatable about an axis, and an extension portion 232 having one end coupled to the column shaft 231 and having a predetermined length. Can be done. In this case, the other end of the extension part 232 may be provided with a mounting holder so that the scan nozzle 220 may be fastened or separated from the holder, or the extension part 232 and the scan nozzle 220 may be integrally formed. have.
  • the extension part 232 may be formed to extend in the longitudinal direction. That is, the scanning nozzle 220 is movable by the scanning arm 230 having the above-described configurations so that the front surface of the wafer can be scanned.
  • the direction of the wafer scanning stage and the nozzle are arranged in an opposite direction, and there is a nozzle at the bottom, and the wafer surface is configured at the top to perform scanning. That is, the scanning nozzle may be configured at the lower portion and the scanning stage may be configured at the upper portion, and the nozzle and the wafer may be vertically scanned.
  • the scanning arm 230 transports the scan nozzle 220 such that the nozzle tip 222 is located close to the center of the wafer w. At this time, the nozzle axis of the scan nozzle 220 is perpendicular to the wafer (w) plane. Thereafter, the scan solution is supplied through the flow path 221 formed in the scan nozzle 220, and the supplied scan solution is agglomerated in the form of droplets on the nozzle tip 222 to contact the surface of the wafer w.
  • the scan stage 210 is slowly rotated with respect to the center point, and the ions of the surface of the wafer w in contact with the scan solution are absorbed into the scan solution.
  • the column axis 231 of the scanning arm 230 rotates at a predetermined angle, and the scanning stage 210 rotates once again, thereby completing scanning to the edge of the wafer w. do.
  • the sample solution scanning the wafer w with the scan solution is transferred to the analysis unit 300 through the flow path 221.
  • the side and back surfaces of the wafer do not act as a direct source of failure, such as contaminants on the upper surface of the wafer, but as a cause of cross-contamination. That is, as the contamination of the inside of the chamber 100, the contamination of the contact part of the transfer robot, etc. act as another contamination source for the wafer to be measured later, in one embodiment of the present invention, after scanning the upper surface of the wafer, The back side is also scanned.
  • FIG. 4 illustrates a process in which the wafer scanning unit 200 scans a side surface of a wafer.
  • the scan nozzle 220 is vertical when scanning the upper surface of the wafer. However, when scanning the side surface of the wafer, the scanning arm 230 is horizontal with the nozzle axis of the scan nozzle 220. It is desirable to redirect the wafer w or the scan nozzle 220 to do so.
  • the scan nozzle 220 as described above.
  • the nozzle axis and the wafer plane are horizontal so that the droplets of the nozzle tip 222 are in contact with the wafer side.
  • a wafer side scan is performed after the scan nozzle 220 and the wafer are disposed.
  • One flow may be formed by communicating flow paths between the scanning nozzle and the analyzer, but as shown in FIG. 15, the solution scanned through the scanning nozzle may be discharged to another reservoir, and the solution stored in the reservoir may be transferred to the analysis unit for analysis. have.
  • the transfer robot may be used to hold both ends of the wafer w loaded on the scan stage 210. After lifting to a certain height, the wafer is inverted up and down. Thereafter, after reloading the wafer as it is on the scan stage 210, the backside of the wafer may be scanned, and contaminant measuring system may be configured through the wafer.
  • the present invention is not limited thereto, and of course, various apparatuses and methods of vertically inverting a wafer may be used. Thereafter, the back side scanning process is the same as the top side measurement process of the wafer.
  • the wafer w which has been scanned to the side and the rear surface as well as the top surface, is transferred by a transfer robot or an operator to be unloaded or stand by a separate wafer cassette (not shown).
  • the measuring method according to an embodiment of the present invention after the scanning and collecting step (S200) step of cleaning the scan nozzle 220 separately from the ion component measuring step (S300) ( S400) may be further performed.
  • the measuring apparatus further includes a nozzle cleaner 400.
  • the nozzle cleaner 400 is provided in the chamber 100 to clean the scan nozzle 220 when the sample solution collected in the scan nozzle 220 is transferred to the analyzer 300. Since the scan nozzle 220 is contaminated while the sample solution containing the ionic contaminant flows, the scanning arm 230 moves the scan nozzle 220 to the nozzle cleaner 400 when the scanning process is completed.
  • the nozzle cleaner 400 is positioned within the rotation radius of the extension part 232 as the column shaft 231 of the scanning arm 230 rotates.
  • the cleaning unit is preferably located within the movement of the XYZ axis.
  • the nozzle cleaner 400 may include a cleaning container 410 in which the scan nozzle 220 is accommodated, and a flow path 420 through which the cleaning solution is drained may be formed at an appropriate position in the cleaning container 410. .
  • FIG. 5 illustrates some cleaning methods in the cleaning step S400 of cleaning the scan nozzle 220.
  • a cleaning solution such as ultrapure water is filled in the cleaning container 410 as shown in FIG. 5 (a).
  • the scan nozzle 220 may be cleaned by applying ultrasonic waves to the cleaning solution using the ultrasonic generator 430.
  • the process of supplying (spraying) and draining ultrapure water into the cleaning container 410 may be repeated.
  • the scan nozzle 220 may be cleaned using the bubbler 440 using a non-contaminating gas such as N2.
  • a drying device (not shown) may be further provided to dry the inert gas without contamination when the cleaning is completed.
  • the cleaning liquid can be automatically analyzed as necessary to manage the degree of contamination.
  • the scanning arm 230 waits the scan nozzle 220 in the nozzle cleaning unit 400 until the control unit receives a movement command for scanning the wafer.
  • the ion component measuring step (S300) is for the purpose of measuring and analyzing the ion component, ion chromatography (IC; Ion Chromatography) or ion chromatography-mass spectrometry
  • IC ion chromatography
  • ion chromatography-mass spectrometry The analysis method of (IC-MS; Ion Chromatography-Mass Spectrometry) can be applied.
  • the analyzer 300 has a large inlet flow path 301, a sample injection valve 310, a sample injection pump 320, a column 330, and a suppressor 340. ) And the detector 350.
  • the scanning solution in which the wafer scanning is completed is sucked by the pump and transferred to the inflow passage 301.
  • the inflow passage 301 communicates with the standard solution injector 20 so that not only the sample solution but also the standard solution for calibration may be transferred. That is, the ion component measuring step (S300) performed by the analyzer 300 determines the component by comparing the time (peak generation time) at which the ions are separated and detected with a preset detection time. Calibration, which is the process of setting the detection time for each reference component in advance using a standard solution already known, should be performed.
  • the path through which the standard solution for calibration is moved and the path through which the sample solution for measurement is moved are the same. Therefore, as calibration conditions and analysis conditions are the same, there is an advantage of preventing fine error of calibration.
  • the sample injection valve 310 includes an eluent, and a sample loop 311 into which one of the standard solution or the sample solution introduced into the inflow passage 301 is injected, and according to the position control command, the sample loop.
  • the flow path connected to 311 is switched.
  • the eluent may be transferred to the column 330 via the sample loop 311.
  • the sample injection pump 320 serves to transfer (load or drain) or inject the sample solution (sample) or standard solution into the sample loop 311.
  • Column 330 is a configuration in which a sample is injected from the sample injection valve 310 to separate the components in the sample. Specifically, when the sample is injected into the sample loop 311 by the loading operation of the sample injection pump 320, the sample injection valve 310 is switched to the injection position and the sample in the sample loop 311 by the eluent injection column 330 is injected into the sample and separation of the sample occurs.
  • the suppressor 340 is configured to lower the conductivity of the background value of the sample, the sample passing through the suppressor 340 is detected by the ion component in the detector 350.
  • the ion component measuring step S300 of the present invention comprises a total of four steps.
  • step 1-1 when the sample injection valve 310 is in the loading position, the sample solution (sample) is moved from the inflow passage 301 toward the sample injection pump 320 by the loading operation of the sample injection pump 320. As the sample is filled in the sample loop (311). Subsequently, the position of the sample injection valve 310 is switched to the injection position by the control unit in step 1-2, and the sample loop 311 as the eluent is injected into the sample injection valve 310 by the eluent injection pump 10. Samples in the sample are transferred to the column 330 to separate the sample.
  • the conductivity of the background value of the sample is lowered by the suppressor 340.
  • the ionic contaminants included in the sample passed through the suppressor 340 by the detector 350 Is detected.
  • the detection method detects the components of the ionic contaminants contained in the sample solution by comparing the detection time (peak generation time) of the components included in the sample with the reference detection time for each component set at the time of calibration as described above. do.
  • the inlet flow passage 301 is divided into two lines on the drawing is a multi-channel analyzer (required) provided with two sample injection valve 310, column 330, the suppressor 340, two detection unit 350 (necessary) According to the sample injection pump 320 may be provided, respectively), but it can be configured as a single channel provided with one configuration each, of course.
  • Figure 6 shows a second embodiment of the ion component measurement step (S300) of the present invention.
  • the measurement method according to the second embodiment of the present invention is to enable automatic sample storage with measurement and analysis of a sample.
  • the analysis unit 300 includes a delay coil 360 and a sample storage ( 370 is further included.
  • the delay coil 360 is configured to fill a predetermined amount of the sample solution loaded from the inflow passage 301 by the loading operation of the sample injection pump 320, and between the sample injection valve 310 and the sample injection pump 320. It is preferable to be provided in the flow path.
  • the delay coil 360 refers to a configuration for storing the sample on the flow path, the flow path in which the fluid flows can act as a delay coil, or a separate flow path storage chamber or coil installed on the flow path It may be.
  • the sample reservoir 370 is provided in communication with a flow path between the inflow passage 301 or the inflow passage 301 and the front end of the delay coil 360, and is opened and closed by a valve. When the valve is opened, the sample solution stored in the delay coil 360 is drained and stored by the drain operation of the sample injection pump 320.
  • step 1 the sample solution introduced from the wafer scanning unit 200 through the inflow passage 301 is loaded into the delay coil 360 by the loading operation of the sample injection pump 320 (arrow 1).
  • step 2 the valve in front of the sample reservoir 370 is opened, and the sample solution filled in the delay coil 360 by the drain operation of the sample injection pump 320 flows into the sample reservoir 370 and is stored.
  • each sample reservoir 370 may be provided for each channel, the sample solution stored in the delay coil 360 divided into two sample reservoirs 370 to be stored (Arrows 2 and 3).
  • the sample stored in the sample reservoir 370 of one of the two channels is loaded into the sample injection pump 320 and then injected into the sample loop 311 of each channel, thereby allowing the two channels to measure and analyze the same sample. have.
  • the front end of the delay coil is provided with a flow control valve 380
  • the flow control valve 380 is a valve for controlling the flow of fluid in two or more directions. Although it is provided in the front end of the delay coil in the drawing, but may be provided at the rear end of the delay coil or both the front end and the rear end, at least one or more to be provided in the flow path between the sample injection valve 310 and the sample injection pump 320 Can be.
  • the flow control valve 380 is also connected to the discharge passage 381, it is possible to discharge the solution as needed.
  • the discharge flow path 381 may be used for the purpose of discharging the solution or the gas after cleaning the flow path in which the sample solution flows after the sample storage or analysis using ultrapure water or high purity gas.
  • the sample solution stored in the sample reservoir 370 is analyzed after a predetermined time, or collected by an operator and analyzed by a separate analysis device or used for other purposes.
  • the control unit when the sample scanning the contaminants from the wafer is in a condition that cannot be analyzed for the same reason as the failure of the detector, the control unit does not transfer the sample to the detector side, but to the sample storage 370. To be automatically saved. Samples that have been scanned once are very important because they are one-time samples that cannot be obtained again. Therefore, when the analysis is impossible or the analysis conditions are incorrect and accurate analysis is difficult, by automatically storing the sample, there is an effect that can prevent data loss.
  • the sample is not automatically measured by the operator's command and stored in the sample storage 370, so that the sample may be analyzed by another analyzer other than the automatic measurement by the analysis unit 300, or when the sample is to be used for other purposes. There is an advantage to recover.
  • Figure 7 shows a third embodiment of the present invention
  • the third embodiment of the present invention is to enable the automatic storage of the sample as in the second embodiment described above, a plurality of sample storage 370 is provided Sample storage is possible in the sample storage 370, and a method of cleaning the flow path will be described.
  • one or more sample reservoirs 370 or standard solution injectors 20 may be provided.
  • a plurality of sample reservoirs 370 are provided, and one sample is used per wafer to maintain inherent contamination characteristics of the wafer, and different sample solutions for each wafer are stored in each sample reservoir 370. It is desirable to.
  • the standard solution injector 20 may also be provided in plural to enable the injection of standard solutions of different concentrations, and the standard solution injector 20 and the sample reservoir 370 may be arranged side by side.
  • a selection valve 390 is further provided between the plurality of standard solution injectors 20 and / or the sample reservoir 370.
  • the selection valve 390 receives a control signal and selectively communicates the interruption portion of the inflow passage 301 with any one of the plurality of standard solution injectors 20 or the sample reservoir 370.
  • the selector valve 390 may include a fixed channel 391 which communicates with a stop of the inflow channel 301, a unit valve 392 provided on the fixed channel 391, and a unit valve 392 and a standard solution.
  • a movement passage (393) which is installed so as to automatically move more than one axis of the XYZ axis. Therefore, by controlling the unit valve 392 and the moving passage 393, the desired standard solution injector 20 or the sample reservoir 370 can be selected.
  • the moving channel 393 is moved to connect with the standard solution inlet 20 having a desired concentration, and the unit valve 392 provided in the fixed channel 391 is connected. Open the standard solution may be introduced into the sample injection valve (310).
  • the selection valve 390 may be used without limitation as long as it is for selectively connecting any one of the flow path and the plurality of storage units as described above, and any one of a solenoid valve, a selection valve, and an auto sampler may be used. Can be.
  • sample reservoir 370 and the standard solution injector 20 may be individually positioned and controlled through respective valves.
  • the flow path through which the sample solution flows or the flow path after the sample solution flows is cleaned.
  • the flow path connected to the delay coil 360 and the sample reservoir 370 may be contaminated in a process in which the sample solution is drained and stored in the sample reservoir 370 when other foreign substances exist.
  • a process of cleaning the flow path by injecting ultrapure water or high-purity gas into the flow path through which the sample solution will flow and then discharging the fluid.
  • the flow control valve 380 is located between the sample injection valve 310 and the sample injection pump 320, and is connected to the ultra-pure water injection unit 30 is injected ultra-pure water to control the ultra-pure water injection Can be.
  • a high purity gas may be injected instead of ultra pure water.
  • the ultrapure water or the high purity gas is injected into one of the sample reservoirs 370, and the selection valve 390 is controlled to load the ultrapure water or the high purity gas of the sample reservoir 370 through the sample injection pump.
  • the discharge flow path 381 of the control valve 380 is discarded.
  • the ultrapure water is loaded from the ultrapure water injection unit 30 through the control of the flow control valve 380 to the sample injection pump 320 and then drained to the sample storage 370. At this time, the drained solution (or gas) is dumped to the drain port next to the sample reservoir 370.
  • the delay coil is a communication flow path for sucking the sample, it can be replaced by a general flow path.
  • the surface of the wafer loaded on the scan stage is scanned to collect ionic contaminants.
  • the ultrapure water is loaded from the ultrapure water injection unit 30 by the sample injection pump 320 (high purity gas is also possible) and the flow path is cleaned up to the selected sample storage 370.
  • the sample in which the contaminants are collected is loaded into the delay coil 360 by the loading operation of the sample injection pump 320, and any one selected from the sample reservoir 370 is opened as the selection valve is controlled.
  • the sample solution filled in the delay coil 360 is introduced into the connected sample reservoir 370 by the drain operation of the sample injection pump 320 and stored. Thereafter, after cleaning the path through which the sample solution was flowed, a new wafer may be loaded and the above process may be repeated.
  • the sample solution scanned the wafer, but is loaded by the sample injection pump 320 as in the first embodiment
  • the sample filled in the delay coil 360 may be injected into the sample loop 311 so that the ions contained in the sample may be measured and analyzed by the column 330, the suppressor 340, and the detector 250.
  • the sample storage step may be further performed separately from the ionic component measuring step.
  • the sample storage step if the sample remains in the delay coil 360 after measuring the ionic component of the sample, the remaining sample may be stored in the sample storage 370 as needed, or the delay coil 360 may be measured before the ionic component measurement.
  • the delay coil is used as a connection flow path, in addition to the method of confining the sample to the delay coil, the sample is injected into the syringe pump 320b and loaded into the sample storage 370 to store the sample, or the sample is injected and then the sample The sample may be injected directly into the sample loop through the injection valve 310.
  • the sample injection pump 320 of the analysis unit 300 may be formed of a first sample injection pump 320a and a second sample injection pump 320b.
  • the first sample injection pump 320a is provided to allow the fluid in the inflow passage 301 to be loaded through the sample injection valve 310 as in the previous embodiments.
  • the second sample injection pump 320b communicates with the stop portion of the inflow passage 301 and is connected to allow the fluid in the inflow passage 301 to be immediately loaded.
  • a selection valve 390 connected to the sample reservoir 370 may be provided between the inflow passage 310 and the second sample injection pump 320b to enable automatic storage of the sample, in which case the selection valve 390.
  • the delay coil 360 is preferably provided between the second sample injection pump 320b.
  • the delay coil may be a connection flow path, and the sample may be injected into the sample injection valve 310 after loading the automatic storage sample into the sample injection pump 320. In this case, the sample is injected for the next sample analysis after loading the sample. It is desirable to flush the pump with ultrapure water.
  • the sample is filled in the sample loop 311 by the loading operation of the first sample injection pump 320a as in the first embodiment, and finally The detector 350 may detect the ion component.
  • the sample introduced into the inflow passage 301 by the second sample injection pump 320b is loaded into the delay coil 360, and the selection valve 390 is controlled to control the desired sample storage ( When the 370 is opened, the sample of the delay coil 360 is drained and stored in the selected sample storage 370.
  • the flow control valve 380b described above is provided between the inflow passage 310 and the second sample injection pump 320b, as shown in FIG. 8, to load a sample or to introduce ultrapure water or N2 to flow path cleaning. Can be used, and the fluid can be drained 381b (also in FIG. 10).
  • FIG. 9 is a fifth embodiment of the present invention, when a sample scanned a wafer flows into the inflow passage 301, it is loaded / drained by the second sample injection pump 320b and stored in the sample storage 370 (FIG. 9 (a)). Thereafter, the sample stored in the sample reservoir 370 is injected into the sample injection valve 310 through a separate flow path L to be measured and analyzed (FIG. 9 (b)).
  • the flow path (L) is also configured to selectively connect the desired sample storage 370 of the plurality of sample storage (370).
  • the sample injection pump 320 is composed of only the second sample injection pump 320b described in the above embodiments, the inflow passage 301 and the second sample injection pump Selection valves 390 and delay coils 360 are sequentially provided between the 320b.
  • the sample solution introduced into the inflow passage 301 is loaded into the delay coil 360 by the second sample injection pump 320b. Drained and injected into the sample injection valve 310 may be measured and analyzed.
  • the valve 312 provided at the front end of the sample injection valve 310 is closed at the time of sample loading of the second sample injection pump 320b, and the sample is opened when the sample is drained for analysis.
  • the sample loop 311 of the sample injection valve 310 is filled from 360 and then discarded into the discharge passage 381a.
  • the sample filled in the sample loop 311 is injected into the column 330 and separated, and after the conductivity background value is lowered, the ionic component is detected by the detector 350.
  • the position of the valve 312 may be installed on the inflow passage 301 of the front end of the sample injection valve 310, it is to be installed on the rear end of the sample injection valve 310, that is, the discharge flow path (381a). It may be.
  • the sample filled in the delay coil 360 may be stored in the desired sample storage 370 through the control of the selection valve 390, the operation description thereof is the same as described above and will be omitted. Meanwhile, the valve 312 should be closed when the sample is drained into the sample reservoir 370.
  • the analysis unit 300 has the delay coil 360, the flow control valve 380, the discharge passage 381, the second discharge passage 302, and the ultrapure water injection. It further comprises a portion 30.
  • Delay coil 360 is provided between the sample injection valve 310 and the sample injection pump 380, the flow control valve 380 is also provided with at least one between the sample injection valve 310 and the sample injection pump 380. It is also connected to the discharge passage 381.
  • the ultrapure water injection unit 30 and the second discharge passage 302 are in communication with the inlet passage 301, and are respectively opened and closed by an on-off valve.
  • example dilution the ionic component measuring steps according to the seventh exemplary embodiment (sample dilution) of the present invention will be described in order with reference to FIG. 11, and may be performed in eight steps.
  • the ultrapure water is loaded into the delay coil 360 by the loading operation of the sample injection pump 320 from the ultrapure water injection unit 30 in the first step.
  • the opening / closing valve of the ultrapure water injection unit 30 is closed in a subsequent step, and the sample solution is transferred from the wafer scanning unit 200 to the ultrapure water by the sample injection pump 320.
  • it is loaded to fill the rest of the delay coil 360 and the sample loop 311. That is, as shown in the figure, when the delay coil 360 is rotated 90 degrees counterclockwise, the front portion (A) is in a state where the sample solution is filled with the ultrapure water (B) at the rear portion.
  • step 3 the flow control valve 380 is controlled to open the discharge flow path 381, and the sample injection pump 320 is switched to the drain operation, so that some of the solution of the delay coil 360 is discharged to the discharge flow path 381. After the discharge, the discharge passage 381 is closed.
  • the ultrapure water and the sample solution are filled in a predetermined ratio on the sample loop 311 by the drain operation of the sample injection pump 320. That is, when the discharge passage 381 is closed after the partial solution (A zone) of the lower side of the flow control valve 380 is discharged in the previous three steps, the remaining solution (B zone) of the delay coil 360 is ultrapure water, and flow control The upper flow path of the valve 380 is filled with the sample solution. Therefore, when the drain operation of the sample injection pump 320 is controlled, ultrapure water and a sample solution may be filled on the sample loop 311 at a desired ratio (C to D). In this case, the sample solution filled on the inflow passage 301 and the sample injection valve 310 in the second step is drained and discharged through the second discharge passage 302.
  • step 5 is a step in which the sample in the sample loop 311 is transferred to the column 330 and separated as the eluent is injected.
  • step 6 the conductivity of the background value of the sample is lowered by the suppressor 340.
  • step 7 ionic components included in the sample are detected.
  • step 8 the detection result is corrected by reflecting the dilution ratio in step 4 to the result detected in step 7, thereby finally measuring the components and concentrations of the ionic contaminants in the sample solution.
  • the dilution method there is a method using the sample reservoir 370 described above as a dilution container. That is, the sample reservoir 370 is provided as shown in FIGS. 6 to 10, and a predetermined amount of ultrapure water and a sample sample are respectively injected into the sample reservoir 370 at a desired ratio and diluted. Thereafter, the diluted sample of the sample reservoir 370 is measured and analyzed in the same manner as in the other embodiments described above, and finally, the detection result is corrected to reflect the dilution ratio.
  • a separate device for supplying a quantitative supply of ultrapure water or separately installed, or the sample injection pump 320 to the ultrapure water and the sample as shown in FIGS. ) Or the delay coil 360, and the injection amount may be automatically calculated according to a dilution ratio set in advance.
  • FIG. 12 illustrates a process for measuring ionic components according to an eighth embodiment of the present invention.
  • the eighth embodiment concentrates and analyzes a sample having a very low concentration. Since the process is relatively simple, it will be briefly described with reference to FIG. 12.
  • the configuration of the analysis unit 300 is similar to the first embodiment (Fig. 1), but further includes a concentrated column 331. That is, the sample solution in the sample loop 311 is concentrated in the concentration column 331 before being transferred to the column 330 and then transferred to the column 330 for separation of the sample.
  • the concentration of the pollutant may be very high or low when a specific process is performed, or the concentration may be roughly determined based on previous measurement results.
  • the sample solution is diluted with ultrapure water at a predetermined rate and diluted before analyzing the components and concentration of the sample solution, and then transferred to the column 330 or the sample solution is concentrated in a column ( 331 is injected and concentrated, and then transferred to the column 330.
  • This increases the accuracy of the measurement by allowing more uniform concentrations of sample solutions to be measured, and in the case of concentrated analysis, there is an advantage in that even trace contamination can be measured.
  • the detector 350 corrects the detection result by reflecting the dilution or concentration ratio in the detection result.
  • the pollutant measuring apparatus is provided with various sensors (not shown) for each predetermined position of the analysis unit 300, the control unit to measure the measured values of the sensors and the previous measurement results of the detector Based on this, various parameters can be monitored. In this case, when at least one of the parameters deviates from the set reference value, each device is controlled to return to the load port without scanning the wafer or to automatically store the sample solution collected by scanning the wafer without analyzing the sample solution.
  • the parameters are pump pressure, conductivity background value, the detection time of the ions, the detection time of the matrix peak, the position of the sample injection valve 310, the temperature of the column 330, the temperature of the detector, the sample transfer sensor It may be any one or more selected from the measured value, the position of the sample infusion pump.
  • the matrix peak means a peak detected by the matrix component.
  • ultrapure water becomes a matrix component when a solution in which various components are dissolved in ultrapure water in an ionic state is used as a standard (same sample).
  • Ultrapure water is a solution from which ions have been removed, and thus low conductivity results in negative peaks, which are called matrix peaks.
  • the matrix peak may be a positive peak or negative peak depending on the properties.
  • the sample solution of the previous wafer is measured, and the detection unit 350 compares the detection time of the ions with the reference detection time. Either no scan is made, or the sample solution is waited without measuring after the scan. You can then recalibrate or analyze the instrument and continue with the measurement.
  • the pollutant measuring method according to the sixth embodiment of the present invention may further comprise a monitoring step.
  • 13 and 14 are flowcharts illustrating a parameter monitoring process of the present invention.
  • the contaminant measuring method according to the ninth embodiment of the present invention includes a wafer loading step (S100 '), a scanning and collecting step (S300'), and an ionic component measuring step (S400 ') like other embodiments.
  • a primary monitoring step S200 ′ in which various parameters are monitored by the controller based on the measured values of the various sensors and the previous measurement result of the analyzer 300. ) Is further included.
  • the loaded wafer is returned to the load port without being scanned or taken out. Or, if necessary, the wafer is scanned to collect the sample solution (when parameters related to the wafer scan are within the set reference values), and the collected solution is automatically transferred to the sample reservoir without storage and measurement.
  • next step may be performed without any special matters, such as wafer scanning and collection, and ionic component measurement and analysis by an analysis unit.
  • the measurement method shown in FIG. 14 further includes a secondary monitoring step in addition to the primary monitoring step. That is, the wafer loading step (S100 ′′), the first monitoring step (S200 ′′), including the scanning and collecting step (S300 '') and the ion component measuring step (S500 '), but the scanning and collecting step (S300') ') And further includes a secondary monitoring step (S400 ′′) in which the parameters are monitored by the controller in the same manner as the above-described primary monitoring step (S200').
  • the sample solution in which the contaminants have already been collected is not stored in the scanning and collecting step without analyzing the sample solution. It is then performed.
  • Contaminant measuring apparatus and method of the present invention is designed for the purpose of measuring and analyzing ionic contaminants, unlike conventional apparatus for analyzing metallic contaminants on the wafer surface.
  • ionic contaminants such as NH 4 + and Cl ⁇ remain on the wafer surface from the chemical used in the process or from the air.
  • the conventional metallic contaminant analyzing apparatus removes the oxide film on the surface of the wafer through a gas phase decomposition unit or the like, and thus, there is a problem in that the ionic contaminants are unsuitable as described above.
  • the present invention does not have a gas phase decomposition unit, and by having an analysis unit 300 capable of analyzing ionic components, there is an advantage that can measure the ionic contaminants present on the wafer surface. That is, since pollutants can be monitored in near real time, there is an advantage in that the yield of semiconductor devices can be greatly improved by reducing defects of semiconductor devices.
  • discharge passage 310 sample injection valve
  • sample loop 320 sample injection pump
  • selection valve 391 fixed flow path
  • the present invention can be used to monitor contaminants on the wafer surface in the production process of semiconductor devices.

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Abstract

La présente invention concerne un appareil et un procédé de mesure de contaminants ioniques adsorbés ou restant sur la surface d'une tranche pendant un processus, l'appareil comprenant : un étage de balayage sur lequel la tranche est chargée dans un état dans lequel une décomposition en phase vapeur de la tranche n'est pas effectuée ; une partie de balayage de tranche pour balayer et prélever, à l'aide d'une buse de balayage, les contaminants ioniques sur la surface de la tranche lorsque la tranche est chargée ; et une partie d'analyse pour analyser les contaminants ioniques contenus dans une solution d'échantillonnage collectée par la partie de balayage de tranche. Ainsi l'appareil peut mesurer des contaminants ioniques tels que le NH4+ et le Cl-, qui sont présents sur la surface d'une tranche pendant un processus de traitement de semi-conducteurs.
PCT/KR2017/006313 2016-06-16 2017-06-16 Appareil et procédé de mesure de contaminants ioniques sur la surface d'une tranche WO2017217804A1 (fr)

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CN113533489A (zh) * 2021-08-09 2021-10-22 上海富乐德智能科技发展有限公司 一种半导体设备零部件通孔内微污染的测试方法
CN117393452A (zh) * 2023-12-11 2024-01-12 合肥晶合集成电路股份有限公司 采集晶圆表面金属的方法
CN117393452B (zh) * 2023-12-11 2024-03-22 合肥晶合集成电路股份有限公司 采集晶圆表面金属的方法

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